Process for the preparation of mannite from natural musts.



GASTON PHILIPPE GUIGNARD, OF MELUN, FRANCE.

PROCESS FOR 'JfH-E PREPARATION OF MANNITE FROM NATURAL IVL'U'S'JTS.

N0 Drawing.

To all whom it may concern:

Be it known that I, GASTON'PHLLIPPE GUIGNARD, a citizen of the Republic of France, and a resident of A'venue des Mar also known to prepare mannite by fermen-' tat-ion from artificial musts, but the net cost of this mannite is extremely high.

The present invention consists of a process for the preparation of mannite from natural musts containing polyglucosides adapted to yield levulose by hydrolysis.

The process of the present invention comprises two principal parts: I. The process of effecting the fermentationof the natural musts in conditions such that they afford the maximum yield; 11. The-process of separating the mannite so produced from the many products contained w'ith it .in the natural musts. a

The natural musts to which the process of the present invention may be'applied are in general all those derived from saccharine juices containing levulose, either naturally or by the inversion of a polyglucoside.

The following description relates to-the application of the process of the present in-, 'v'ention to the most difficult case, that is to say the preparation of mannite from beet-- root musts: v

I. ermentatz'o'n of the'natttral must.

' In order to obtain mannite economically, it is necessary to start from beet-roots as rich in sugar as possible. On the other hand in order that the mannitic fermentation may give the maximum yield of mannite, it is necessary for the must to contain at least 150' grams oflevulose per liter. The beet must is first of all prepared byany of the usual known -methods; mineral acid, preferably sulfuric, is then added, and the whole is brought to boiling in such a way as to Specification of Letters Patent.

Patented Mar. 14, 1916.

Application filed March 5, 1913. Serial No. 752,217.

'invert the sugar. The total inversion once produced, an excess of carbonate preferably carbonate of lime is added in order to neutralize the liquid There is then added a certain quantity of brewers? yeast, about 7 kilograms per hectoliter of must. This yeast has preferably been first suspended in a small quantity of boiling Water and maintained at boiling for half an hour so as to be completely killed. After the addition of the yeast, the 'must is concentrated so as to obtain the desired richness in levulose. This concentration takes place in oacuo, and almost half of the water contained in the must is removed. The concentrated must is,

thenv sterilized at 120 degrees C. andfer- I of which aflects the, life of the ordinary mannitic ferment. It is, therefore, necessary to accustom or acclimatize the ferment to the must in which it is to live To obtain the best results, it is advisable to fertilize the natural must only with a ferment accustomed to live in a more concentrated must. The accustoming or acclimatizing of the ferments is effected in the following manner The mannitic ferment derived from cultures upon concentrated artificial musts serves for the fertilization of a beetroot must prepared as stated above but of very low concentration. This ferment serves for the fertilization of a second beetroot must more concentrated than the first and so until the ferment has served for the fertilization of a mustof higher concentration than the principal must to be treated. The ferment accustomed in this Way can be utilized with certainty of success for the fer: tilization of the principal must.

Fermentation of the principal must-Juvert sugar consists, as is known, of glucose and levulose. The mannitic ferment yields With these'two substances the following series of compounds :(a) With levulose:-

mannite, acetic acid,lactic' acid, glycerin, succinic acid, carbonic aid. (7)) IVith glucose: ordinary alcohol, lactic acid, acetic acld, glycerin, carbonic acid. Fermentation takes place in sterilized vats, closed and protected from entrance of air. All possible precautions in construction must be taken in order ,toavo-1d contamination. The carbonic and of lime, alkaline malat'es, lactate of lime,

acetate of lime, glycerin, nitrogenoussubstances soluble in alcohol,var1ous saline substances derived from the musts,

, Manniteis hardly at all soluble in cold alcohol; advantage is taken of this property to operate in the following manner :Alcohol is saturated while cold withmannite and the dried vinasse is washed with this alcohol, which dissolves the glycerin, the nitrogenous substances soluble in alcohol andthe alkaline malatesl The residue of the washing, freed from alcohol by heat, is taken up in' water and ferrous sulfate is then added, The lactate and acetate of lime are transformed into ferrous lactate and acetate insoluble in hot alcohol. The lime passes into the state of sulfate. The mass is evaporated afresh to dryness, then washed with hot al ,cohol which dissolves the mannite alone;

the latter is precipitated by cooling.

' .The process of the present invention is suitable for the treatment of all natural musts containing levulose, with if necessary certain'mo'dificationsof'detail which vary with, the nature of the musts and are evident to one skilled in the art. 7

Having now particularly described and ascertained the nature of my said invention and in what manner the same is to be performed, I declare that what I claim is 1.- In' the process of'obtaining mannite from natural musts, the steps of fertilizing inverted, neutralized, concentrated and sterilized natural-musts having at least 150, grams of levulose per liter by means of. mannite ferments previously accustomed to live inlnatural musts of higher concentration than the must under treatment, fermenting the thus fertilized must, and separating'the mannite produced by this fermentation of the mass. v

' 2. In the process of obtaining mannite "from natural musts, the steps of fertilizing inverted,;neutralizedflconcentrated and sterilized natural-"musts having at least 150 grams of levulose per lite'rzby means of mannite ferments previously gradually accustomed step by step to live in natural musts of higher-concentration than the must under treatment, fermenting the thus fertilized must, and separating the mannite produced by this fermentation of the mass. 3. In the process \of obtaining mannit from natural musts, the steps of fertilizing inverted, neutralized, concentrated and sterilized natural musts by means of mannite ferments previously accustomed to live in natural-musts of higher concentration than the .must under treatment, fermenting the thus fertilized must, distilling oil the alcohol produced by this fermentation, desiccating the remaining vinassei, washing the latter with cold-alcohol saturated with mannite,

evaporating the alcohol from the residue, dissolving the residue in water, adding fer rous sulfate, evaporating to dryness, washing with hot alcohol to dissolve mannitealone and precipitating the mannite therefrom by cooling; r 4; In thetprocess of obtaining mannite from natural musts, the steps of fertilizing I inverted, neutralized, concentrated and ster ilized natural musts havingat least 150 grams of levulose per liter by means, of a mannite ferment previously" accustomed to live in natural musts of higher concentration thanthe must under treatment, for the purpose described. I

5. In theprocess of obtaining mannite from natural musts, the step of fertilizing natural musts by means of amanniteferment previously accl'imatized to a must having more than grams'of levulose per liter."

6. In the process of obtaining mannite from natural musts, the step of fertilizing natural musts, having at least 150. grams of levulose p'er liter, by means of a mannite fermentacclimatized to a. must'having. a higher concentration than the must under treatment. In testimony whereof I have signed my name to this specification, in the presence-of two subscribing witnesses;

GASTON PHILIPPE GUIGNARD.

Witnesses: I

JA UEs LEJEUNE, FERNAND GRIVAULT. 

